Direct determination of Cu, Cd, Ni and Pb in aquatic humic substances by graphite furnace atomic absorption spectrometry

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Voltammetric determination of isoprenaline in pharmaceutical preparations using a copper(II) hexacyanoferrate(III) modified carbon paste electrode

The electroanalytical determination of isoprenaline in pharmaceutical preparations of a homemade carbon paste electrode modified with copper(II) hexacyanoferrate(III) (CuHCF) was studied by cyclic voltammetry. Several parameters were studied for the optimization of the sensor such as electrode composition, electrolytic solution, pH effect, potential scan rate and interferences in potential. The optimum conditions were found in an electrode composition (in mass) of 15% CuHCF, 60% graphite and 25% mineral oil in 0.5 mol l(-1) acetate buffer solution at pH 6.0. The analytical curve for isoprenaline was linear in the concentration range from 1.96 x 10(-4) to 1.07 x 10(-3) mol l(-1) with a detection limit of 8.0 x 10(-5) mol l(-1). The relative standard deviation was 1.2% for 1.96 x 10(-4) mol l(-1) isoprenaline solution (n=5). The procedure was successfully applied to the determination of isoprenaline in pharmaceutical preparations; the CuHCF modified carbon paste electrode gave comparable results to those results obtained using a UV spectrophotometric method. (C) 2004 Elsevier B.V. All rights reserved.

Infecção hospitalar associada ao uso de cateter venoso central e a quebra de protocolos pelos profissionais de saúde na UTI de um hospital universitário em Natal/RN

This is a study descriptive cross-sectional and quantitative approaches, which aimed to analyze the association between hospital infection rate for insertion, maintenance of central venous catheter and the breakdown of protocols (rules and routines) by health professionals assisting patients in the ICU of a university hospital in Natal / RN. The process of data collection was through observation with structured form, refers to medical records and structured questionnaires with health professionals. The results were organized, tabulated, categorized and analyzed using SPSS 14.0. The characterization of the subjects was performed using descriptive and inferential statistics, taking into account the nature of the variables, with analysis of variance (ANOVA) and Spearman correlation test, it was a discussion of the information obtained, considering the mean, standard deviation, coefficient of variance and standard error. The variables that showed a higher level of correlation were treated with the application of significance tests. As the results, 71% of participants were female and 29% male, age ranged from 18 to 85 years (52.6 ± 22.5). The insertion, there was a variation from 0 to 5 errors (1.2 ± 1.4), during maintenance, the average was 2.3 ± 0.9 errors, ranging from 0 to 4. During the insertion and maintenance of CVC, patients who had been an infection ranging from 2 to 9 mistakes (4.2 ± 1.7), since those who did not show the variation goes from 0 to 5 errors (2, 8 ± 1.5). The correlation coefficient between the risk of infection throughout the process and the risk of infection at the insertion showed strong and significant (r = 0.845 p = 0.000) and in relation to risk of infection in maintenance was moderate and significant (r = 0.551 p = 0.001). The mistakes made by professionals in the procedures for insertion and maintenance of the catheter, associated with other conditions, shown as a risk factor for the of IH

Desenvolvimento e validação de método analítico para determinação de WE010, WE014 e WE017

The synthetic guanylhydrazones WE010 (3,5-di-tert-butil-4-hidroxibenzaldehyde-guanylhydrazone), WE014 (4-bifenilcarboxialdehydeguanylhydrazone) and WE017 (3,4-diclorobenzaldehydeguanylhydrazone) showed high cytotoxic activity in terms of percentage inhibition of cancer cells growth. However, further progress in the development of these drug candidates requires precise and convenient methods for their qualitative and quantitative analyses. The aim of this study was to develop and validate High Performance Liquid Chromatography with diode-array detection (HPLC-DAD) and Ultra Fast Liquid Chromatography with diode-array detection (UFLC-DAD) methods suitable for as simultaneous as isolated determination of studied guanylhydrazones, based on the optimization of chromatographic parameters and obtaining reduced detection times. The chromatographic analyses of analytes by HPLC were performed on C18 ACE analytical column (150 mm x 4.6 mm), with a particle size of 5.0 μm. Among all the conditions assayed, the best results of separation were obtained with a mixture of methanol:water (60:40, v/v) as the mobile phase at a flow rate 1.5mL/min and pH of 3.5 adjusted at acetic acid. The UFLC method was developed by experimetal desing techniques in order to find optimal chromatographic analytical conditions, which were achieved on XR-ODS analytical column (50 mm x 3.0 mm), with a particle size of 2,2 μm, maintained at 25 ºC. The mobile phase was consisted of methanol:water (65:35, v/v) with 0.1% triethylamine (TEA) and pH of 3.5 adjusted at acetic acid, at a flow rate 0.5 mL/min. The procedure were validated following evaluating parameters such as specificity, linearity, limits of detection (LD) and quantification (LQ), precision, accuracy and robustness, giving results within the acceptable range. Although the UFLC method shows better sensitivity (lower values of LD and LQ), robustness (lower rates of relative standard deviation) and minimize spending time and solvent, both developed methods were adequately applied to the analysis of guanylhydrazones molecules, may be used in routine of quality control laboratories. Keywords: guanylhydrazones, HPLC/DAD, UFLC/DAD, validation of analitical method

Seleção para peso pós-desmama em um rebanho Gir. 1. Resposta direta e correlacionada em 21 anos de seleção

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Results of 23 years of selection for post-weaning weight in a Caracu beef herd

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Balanço de radiação e energia da cultura de alface em estufa de polietileno

Objetivou-se, neste trabalho, determinar os balanços de radiação e energia da cultura de alface (Lactuca sativa, L. cv. Verônica) em estufa de polietileno. O experimento foi realizado em uma estufa tipo túnel alto com cobertura de polietileno (100 mim de espessura) e em uma área externa, ambas com 35 m². Durante o ciclo da cultura, foram monitoradas as radiações global e refletida, saldo de radiação, fluxo de calor no solo e temperatura do ar (seca e úmida) nos dois meios. Utilizou-se um Datalogger que operou na freqüência de 1 Hz, armazenando médias de cinco minutos. A partir das integrações diárias das irradiâncias global (K¯) e refletida (K­), verificou-se que a transmissividade média da radiação global (K¯in / K¯ex) foi aproximadamente constante, em torno de 79,59%, enquanto a razão das radiações refletidas (K­in / K­ex) foi igual a 69,21% com coeficiente de variação de 8,47%. As curvas normalizadas do saldo de radiação de ondas curtas em relação à radiação global (K* / K¯), nos dois meios, mostraram ser aproximadamente constantes no início do ciclo e decrescentes no final. A relação (Rn/ K¯) foi maior no meio externo, em torno de 12%, a partir da fase em que a superfície verde da cultura cobriu o solo. O balanço médio (L*) de radiação de ondas longas foi maior no exterior, em torno de 50%. O balanço de energia, estimado em termos de fluxos verticais, mostrou, em média, que: no exterior, 83,07% do saldo de radiação foi convertido em calor latente (LE), 18,00% em fluxo de calor no solo (G) e 9,96% em calor sensível (H), enquanto que, no interior da estufa, 58,71% do saldo de radiação foi convertido em LE, 42,68% em H e 28,79% em G.

Agronomic characteristics of 'Prata-anã' and 'Maçã' bananas micropropagated

O experimento foi instalado com o objetivo de estudar o desempenho agronômico de cultivares de bananeira Prata-anã e Maçã, na região de São Manuel-SP. Foram avaliadas as seguintes características de desenvolvimento, no primeiro ciclo de produção: número de dias do plantio à floração e da mesma à colheita, número de rebentos (filhos) emitidos até o surgimento da inflorescência e na época da colheita, número de folhas ativas na época do aparecimento da inflorescência e da colheita, e características de rendimento, como peso médio do cacho, ráquis, penca e fruto, número médio de frutos por penca e cacho, comprimento e diâmetro médio dos frutos. Também foi avaliada a incidência de pragas e doenças. Foi empregado o delineamento inteiramente casualizado, com 2 tratamentos, 15 repetições e 5 plantas úteis por parcela experimental. As duas cultivares foram caracterizadas pelos valores das estatísticas descritivas, média e desvio-padrão, para as características de interesse no experimento. Foram estabelecidas possíveis correlações entre medidas de desenvolvimento e produção. As duas cultivares apresentaram ciclo do plantio até a colheita de 574 dias para 'Prata-anã' e 567 dias para 'Maçã', sendo que o ciclo produtivo foi maior na 'Prata-anã'. Não houve problemas de pragas e doenças em todo o ciclo de produção, nas duas cultivares avaliadas.

Distribuição volumétrica de calda produzidas pelas pontas pulverização XR, TP e TJ sob diferentes condições operacionais

Foram avaliados os perfis de distribuição volumétrica das pontas de pulverização de jato plano Extended Range XR 8004, Teejet TP 8004 e TwinJet TJ60-8004, em mesa de teste construída segundo a norma ISO 5.682-1:1996, sendo as pontas de pulverização posicionadas a 30, 40 e 50 cm de altura da mesa coletora, submetidas à pressão de 200 e 300 kPa, e posicionadas com ângulos de 30 e 45º nos sentidos horário e anti-horário e na posição vertical (0º). As pontas TJ60-8004 foram analisadas nas mesmas alturas, porém somente na posição vertical. Avaliaram-se 10 unidades de cada tipo de ponta, instaladas isoladamente na mesa. A distribuição média do volume pulverizado, coletado nas provetas, foi inserida em programa computacional, que permitiu a simulação do perfil de distribuição de uma barra pulverizadora com 24 bicos, em espaçamentos variáveis, obtendo-se ao final o coeficiente de variação, o desvio-padrão e a média do volume. Os resultados mostraram que a uniformidade de distribuição é menos influenciada pela variação da altura da barra quando o espaçamento entre bicos é reduzido e que há necessidade de adequação do espaçamento quando se utiliza ângulo na barra pulverizadora.

Equilíbrio líquido-líquido para o sistema biodiesel de óleo de semente de melão (Cucumis melo l.) + metanol + glicerina

Rio Grande do Norte, northeast state from Brazil, it is the greatest producer and exporter of yellow melon, well known as Spanish melon. Despite the consumption of this fruit to be mainly its pulp, melon seeds are an important source of lipids considered an industrial residue it has been discharge product. The use of oilseeds in order to produce biodiesel establishes an important raw material and the increase of its production promotes the national development of the agriculture. In this background, the aim of this work has been to use oil from seeds of yellow melon to produce biodiesel and to accomplish a study of the phase equilibrium of the system evolving biodiesel, methanol and glycerin. The biodiesel was obtained by oil transesterification through methylic route with molar ratio 1:9.7 (oil:alcohol) and with a mass of NaOH of 0.5% from the oil mass; the reaction time was 73 minutes at 55 °C. A yield of 84.94% in biodiesel was achieved. The equilibria data present a well-characterized behavior with a great region of two phases. The tie lines indicate that methanol has a best solubility in the phase that is rich in glycerin. Consistency of the experimental data was made based on Othmer-Tobias and Hand correlations which values above 0.99 were found to correlation coefficients, this fact confers a good thermodynamic consistency to the experimental data. NRTL and UNIQUAC models were employed to predict liquid-liquid equilibrium of this system. It was observed a better concordance of the results when NRTL was applied (standard deviation 1.25%) although the UNIQUAC model has presented a quite satisfactory result either (standard deviation 2.70%). The NRTL and UNIQUAC models were also used to evaluate the effect of temperature in the range of 328 K to 358 K, in which a little change in solubility with respect to the data obtained at 298 K was observed, thus being considered negligible the effect of temperature

Application of the Potentiometric Stripping Analysis with Constant Current for the Determination of Lithium Ions Using a Spinel-Type Manganese (IV) Oxide-Modified Carbon Paste Electrode

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Determination of gatifloxacin in bulk and tablet preparations by high-performance liquid chromatography

A sensitive, precise, and specific high-performance liquid chromatographic (HPLC) method was developed for the assay of gatifloxacin (GATX) in raw material and tablets. The method validation parameters yielded good results and included the range, linearity, precision, accuracy, specificity, and recovery. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. The HPLC separation was carried out by reversed-phase chromatography on a C18 absorbosphere column (250 x 4.6 mm id, 5 pm particle size) with a mobile phase composed of acetic acid 50/o--acetonitrile-methanol (70 + 15 + 15, v/v/v) pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 287 nm. The calibration graph for GATX was linear from 4.0 to 14.0 mu g/mL. The interday and intraday precisions (relative standard deviation) were less than 1.05%.

Determination of lomefloxacin in tablet preparations by liquid chromatography

A sensitive, precise, and specific high-performance liquid chromatography (HPLC) method was developed for the assay of lomefloxacin (LFLX) in raw material and tablet preparations. The method validation parameters yielded good results and included the range, linearity, precision, accuracy, specificity, and recovery. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. The HPLC separation was performed on a reversed-phase Phenomenex C18 column (150 x 4.6 mm id, 5 pm particle size) with a mobile phase composed of 1% acetic acid-acetonitrile-methanol (70 + 15 + 15, v/v/v), pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 280 nm. The calibration graph for LFLX was linear from 2.0 to 7.0 mg/mL. The interday and intraday precisions (relative standard deviation) were less than 1.0%. The method was applied for the quality control of commercial LFLX tablets to quantitate the drug.

Microbiological assay for ceftazidime injection

A simple, sensitive, and specific biodiffusion assay for the! antibacterial ceftazidime was developed using a strain of Staphylococcus epidermidis (ATCC 12228) as the test organism. Ceftazidime was measured in powder for injection at concentrations ranging from 100 to 400 mu g/mL. The calibration graph for ceftazidime was linear (r(2) = 1), and the method validation showed that it was precise (relative standard deviation = 0.415) and accurate. The results obtained by biodiffusion assay were statistically calculated by linear parallel model and by means of regression analysis and were verified using analysis of variance. It was concluded that the microbiological assay is satisfactory for in vitro quantification of the antibacterial activity of ceftazidime in pharmaceuticals.

Multivariate optimization and validation of an analytical methodology by RP-HPLC for the determination of losartan potassium in capsules

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)